CN103045885A - Preparation method for high-density fine grain tungsten copper alloy - Google Patents
Preparation method for high-density fine grain tungsten copper alloy Download PDFInfo
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Abstract
The invention relates to a preparation process for high-density fine grain tungsten copper alloy. The alloy consists of 50 to 90 percent of W and 10 to 50 percent of Cu. The preparation process synthesizes the mechanical alloying advantage of ball milling and dry milling and the quick grain refining advantage of wet milling in the aspect of preparation of powder, and also synthesizes the liquid phase rearrangement advantage of liquid phase sintering and the forming pressure-reducing and sintering time-shortening advantages of solid phase hot-pressed sintering in the aspects of sintering process, so the high-density fine grain tungsten copper alloy with the relative density of 99.2 to 99.5 percent and tungsten crystal grain of 0.3 to 0.8 micron is prepared at the relatively low sintering temperature. The tungsten copper alloy prepared by the preparation process is uniform in structure, low in oxygen content, small in crystal grain and high in density; and the process is simple and the used equipment is industrial common powder manufacturing equipment and sintering equipment, so industrialized production is facilitated.
Description
Technical field
The present invention relates to the preparation method of Tungsten-copper Composites, refer to especially the always preparation method of the thin brilliant tungsten-copper alloy of high densification.Belong to the mmaterial preparing technical field.
Background technology
The matrix material that tungsten-copper composite material is comprised of the copper of the tungsten of high-melting-point, low thermal coefficient of expansion and high conductivity, high heat conductance, combine tungsten and copper characteristic separately, therefore, be widely used in electronic package material, heat sink material, vacuum technique and space industry etc.The ideal structure that is used as the tungsten-copper alloy of Electronic Packaging and heat sink material should be high-compactness, and homodisperse tungsten particle forms continuous skeleton, and the Cu that solidifies attitude is filled in the middle of the hole of W skeleton, is continuous three-dimensional communication structure.
Because tungsten and copper are all immiscible under solid-state and liquid state, powder metallurgy is the main technique approach of preparation tungsten-copper alloy material and goods.The preparation technology of conventional tungsten copper alloy has infiltration method, liquid phase sintering and vacuum heating-press sintering etc. at present.Infiltration method is first tungsten powder to be cold-pressed into base, and preliminary sintering is made W skeleton, places copper powder or the copper billet of compacting at skeleton again, rises to high temperature, the copper fusing is infiltrated in the tungsten base space, thereby make Tungsten-copper Composites.Owing in the W skeleton sintering process, form easily closed pore (1% ~ 3%), therefore can not obtain high fine and close tungsten-copper alloy, when W content is low, be difficult to form stable skeleton simultaneously, limited the range of application of the method.Liquid phase sintering mainly is that tungsten powder and copper powder are mixed, and adds tackiness agent and be cold-pressed into base, directly obtains tungsten-copper composite material by liquid phase sintering again under the high temperature more than 1200 ℃.Because the wettability of tungsten and copper is relatively poor, adds a small amount of Ni in order to tend in the densification liquid sintering process, the elements such as Co improve its wettability, yet these elements can make the thermal conductivity of tungsten-copper alloy and electric conductivity reduce.The solid phase hot pressed sintering refers to the W-Cu composite powder is placed in the inertia graphite jig, makes powder be lower than sintering under the temperature of Cu fusing point in pressurization, can within a short period of time sintering obtain uniform goods, be a kind of reinforced sintering method.The great advantage of hot pressing can greatly reduce exactly compacting pressure and shorten sintering time, and the crystal grain of the tungsten-copper alloy of preparing simultaneously is thinner, yet the Cu of solid phase does not almost have flowability, and the density of the tungsten-copper alloy of preparation generally is lower than 98%.
The problem that exists in order to solve traditional technology, studied at present the novel process of many preparation Tungsten-copper Composites both at home and abroad, the common characteristics of these novel procesies are to prepare the superfine W-Cu composite powder with larger sintering activity, prepare high fine and close Tungsten-copper Composites by traditional cold-rolled sintered technique again, preparation method for superfine W-Cu composite powder, mainly contain two kinds of chemical method and mechanical process, wherein chemical method is to tungstenic, the precursor solution of copper forms powder or utilizes precipitation agent to generate throw out by spraying drying, roasting forms the mixture of Tungsten oxide 99.999 and cupric oxide again, then generate the nano-class composite W-Cu powder body by hydrogen reducing, such as patent 200710118440.7,200710024801.1,201110007251.9 etc., though these methods can be prepared the nano-class composite W-Cu powder end, complex procedures, and use or generate corrosives in the process (such as concentrated nitric acid, the vitriol oil, nitrogen peroxide etc.), high to equipment requirements, and cause easily environmental pollution.Mechanical process mainly is to pulverize W-Cu composite powder by high-energy ball milling, such as patent 03143145.3, prepare nanocrystalline W-Cu composite powder by the high energy wet-milling, yet in high energy wet-milling process, because the adding of ball-milling medium and tensio-active agent, easily powder is polluted on the one hand, these reagent form the mechanical alloying that fluid film has hindered tungsten copper at particle surface on the other hand.In addition, in these techniques, all mainly be to produce around generating the nano-class composite W-Cu powder end, sintering process is still according to traditional cold-press moulding liquid sintering technology, sintering temperature is generally more than 1200 ℃, time, also generally more than 2h, it was tiny to be unfavorable for forming crystal grain, the high fine and close tungsten-copper alloy of homogeneous microstructure.
Summary of the invention
The object of the invention is to overcome the deficiency of prior art and provide a kind of technique simple, the tungsten-copper alloy homogeneous microstructure of preparation, oxygen level is low, and crystal grain is little, the preparation method of the high fine and close thin brilliant tungsten-copper alloy that density is high.
The preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification of the present invention may further comprise the steps:
The first step: starting material prereduction is processed
Get respectively the prereduction in hydrogen atmosphere of pure copper powder, pure tungsten powder, the pure copper powder reduction temperature is: 400 ~ 500 ℃; The pure tungsten powder reduction temperature is: 700 ~ 800 ℃; The mean particle size of pure copper powder, pure tungsten powder is 2 ~ 15 μ m;
Second step: ball milling
The first step gained pure copper powder, pure tungsten powder are mixed, place the ball sealer grinding jar, be evacuated to 10
-1~ 10
-2Then Pa, passes into rare gas element to normal pressure in ball grinder; At first, dry grind at a high speed with the rotational speed of ball-mill of 400 ~ 500r/min after; Add the low molecule grinding aid that accounts for ball, material total mass 0.1 ~ 0.2% again in ball grinder, then, the rotational speed of ball-mill low speed wet-milling with 125 ~ 200r/min obtains the nanocrystalline W-Cu composite powder of high solid solution;
The 3rd step: restore
The nanocrystalline W-Cu composite powder of the high solid solution of second step gained is placed hydrogen atmosphere, be heated to 700 ~ 800 ℃, insulation 0.5 ~ 1.0h restores;
The 4th step: sintering
The 3rd step gained powder is packed in the graphite jig, and it is 10 that mould is put into vacuum tightness
-3~ 10
-4In the vacuum hotpressing machine of Pa, temperature rise rate with 10 ℃/min ~ 20 ℃/min rises to 1100 ~ 1150 ℃ from room temperature, after the insulation, rate of temperature fall with 2 ~ 5 ℃/min is cooled to 1050 ~ 1080 ℃, apply the pressure of 40 ~ 50Mpa, heat-insulation pressure keeping 1.0 ~ 2.0h cools to room temperature with the furnace, namely obtains high fine and close thin brilliant tungsten-copper alloy.
The preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification of the present invention, described pure copper powder, pure tungsten powder are technical pure copper powder, technical pure tungsten powder; Its purity is respectively: copper powder purity〉99.7%, tungsten powder purity 99.5%.
The preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification of the present invention, described prereduction soaking time is 0.5 ~ 1h.
The preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification of the present invention, in the second step, it is to adopt mixer to mix 1 ~ 2 hour that described pure copper powder, pure tungsten powder mix.
The preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification of the present invention, in the second step, the ball material mass ratio of described high speed dry grinding and described low speed wet-milling is: 10 ~ 15:1; Described high-speed dry time consuming 10 ~ 20h; Low speed wet-milling time 2 ~ 5h.
The preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification of the present invention, in the second step, described low molecule grinding aid is selected from a kind of in dehydrated alcohol, stearic acid, ethylene glycol, the propylene glycol; Low molecule grinding aid is added in the ball grinder, is to place the glove box of atmosphere of inert gases to open ball grinder, add low molecule grinding aid to ball grinder after, ball sealer grinding jar again.
The preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification of the present invention, in the 4th step, described graphite jig internal surface scribbles releasing agent, and described releasing agent is boron nitride.
The preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification of the present invention, in the 4th step, 1100 ~ 1150 ℃ of sintered heat insulating times are 15 ~ 30min; 1050 ~ 1080 ℃ of heat-insulation pressure keeping times are 1.0 ~ 2.0h.
The preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification of the present invention, the high fine and close thin brilliant tungsten-copper alloy relative density for preparing is 99.2% ~ 99.5%, and tungsten is evenly distributed mutually, and particle diameter is 0.3 ~ 0.8 μ m.
The preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification of the present invention, high fine and close thin brilliant tungsten-copper alloy comprises that following component forms by mass percentage:
Tungsten 50 ~ 90,
Copper 10 ~ 50.
The present invention is owing to adopt above-mentioned processing method, combine the advantage of the grain refine of the mechanical alloying of ball milling dry grinding and wet-milling in powder preparation, on sintering process, also combine the liquid phase rearrangement of liquid phase sintering and the advantage that the solid phase hot pressed sintering reduces compacting pressure and shortening sintering time, preparing relative density under relatively low sintering temperature is 99.2 ~ 99.5%, tungsten grain is 0.3 ~ 0.5 μ m, the high fine and close thin brilliant tungsten-copper alloy of homogeneous microstructure.Ball-milling technology wherein carries out in two steps, and mechanical alloying has namely occured the sosoloid that the high speed dry grinding of the first step can make the tungsten copper System forming have certain solid solubility.The low speed wet-milling of second step can make the powder fragmentation of caking and sticking tank in dry grinding at a high speed and come off, and makes the further refinement of powder of mechanical alloying, forms the nanocrystalline W-Cu composite powder of high solid solution.Follow-up reduction is processed on the one hand and is made the copper of solid solution separate out mutually and be evenly distributed on the tungsten particle surface, can make on the other hand residual grinding aid volatilization, guarantees the low oxygen content of powder, more is conducive to vacuum sintering.In the vacuum sintering process of powder, liquid phase rearrangement occurs in powder in 1100 ~ 1150 ℃ the of short duration insulation that is higher than the Cu fusing point, owing to separate out the wettability that greatly to improve mutually tungsten copper at the copper on tungsten particle surface, tungsten copper powder is densification at short notice, along with temperature is down to (1050 ℃ ~ 1080 ℃) under the Cu fusing point gradually, the flowability of copper weakens, apply less pressure this moment, and (40 ~ 50Mpa) oozing out of copper liquid can't occur, but help the further densification of tungsten-copper alloy, therefore finally just obtain relative density in the short time and reach 99.2% ~ 99.5% tungsten-copper alloy, because lower sintering temperature and short sintering time, the tungsten particle crystal grain of the tungsten-copper alloy that obtains only has 0.3 ~ 0.8 μ m.Use the tungsten-copper alloy homogeneous microstructure of the present invention's preparation, oxygen level is low, and crystal grain is little, and density is high, and technique is simple simultaneously, and equipment all is based on industry often powder process and agglomerating plant, is conducive to suitability for industrialized production.
Description of drawings
The secondary electron pattern of the nanocrystalline W-Cu composite powder of high solid solution that accompanying drawing 1 makes for embodiment 1 mechanical ball milling.
The back scattering pattern of the high fine and close thin brilliant tungsten copper composite alloy that accompanying drawing 2 makes for embodiment 1 vacuum heating-press sintering, wherein color is divided into the tungsten phase than superficial part, is divided into the copper phase than the deep.
Can find out from accompanying drawing 1: the W-Cu composite powder granular size that the process ball milling obtains is about 0.5 ~ 1 μ m, because particle is tiny, the part powder has agglomeration.
Can find out from accompanying drawing 2: tungsten is evenly distributed mutually, and its size distribution is at 0.3 ~ 0.8 μ m.
Embodiment
Embodiment 1: the preparation standard composition is W(85%wt), tungsten-copper alloy Cu(15%wt), its standard density is 16.40g/cm
3, follow these steps to finish:
1. general industry is respectively taken by weighing 60g with pure copper powder (particle diameter is 5 ~ 100 μ m), pure tungsten powder (particle diameter is 2 ~ 15 μ m), 340g in atmosphere of hydrogen under the time of carrying out be that 45min reduction is processed, reduction temperature is respectively 450 ℃, 780 ℃.
2. will mix 2 hours at mixer through copper powder and the tungsten powder that reduction is processed.
3. the tungsten copper mixed powder is put into stainless steel jar mill, add the Stainless Steel Ball (ratio of grinding media to material 15:1) of 6kg, ball grinder is evacuated to 10
-2Pa, pass into again straight argon gas, with the lid sealing, carry out the high-speed dry mill at ball mill, behind the rotational speed of ball-mill ball milling 20h with 450r/min, in the glove box of argon atmosphere, ball grinder is opened, added 40ml dehydrated alcohol and again sealing taking-up to ball grinder, rotational speed of ball-mill ball milling 2h with 100r/min obtains the nanocrystalline W-Cu composite powder of high solid solution.
4. the reduction that with ball milling gained powder time of carrying out in atmosphere of hydrogen is 45min is processed, and reduction temperature is 800 ℃.
5. the ball milling ball-milled powder after will reducing is packed into to cooperate closely and at internal surface and is scribbled in the high-strength graphite mould of releasing agent, and wherein releasing agent is boron nitride.
6. mould is put into vacuum hotpressing machine.10
-310
-4Under the vacuum tightness of Pa, from rising to 1150 ℃, insulation 30min is cooled to 1080 ℃ with the rate of temperature fall of 2 ℃/min, applies the pressure of 50Mpa with the temperature rise rate of 20 ℃/min, and heat-insulation pressure keeping 2.0h cools to room temperature with the furnace.
7. the demoulding: the tungsten-copper alloy ingot is taken out from graphite jig, surface finish, according to dense sintering metallic substance and Wimet density inspect method (GB GB03850), recording the actual density of matrix material is 16.25g/cm
3, relative density=actual density/standard density=99.2% can find out that by the back scattering pattern of metallographic its tungsten is evenly distributed mutually, particle diameter is 0.3 ~ 0.5 μ m.
Embodiment 2: the preparation standard composition is W(70%wt), tungsten-copper alloy Cu(30%wt), its standard density is 14.28g/cm
3, follow these steps to finish.
1. general industry is respectively taken by weighing 280g with pure copper powder (particle diameter is 5 ~ 100 μ m), pure tungsten powder (particle diameter is 2 ~ 15 μ m), 120g in atmosphere of hydrogen under the time of carrying out be that 45min reduction is processed, reduction temperature is respectively 450 ℃, 780 ℃.
2. will mix 2 hours at mixer through copper powder and the tungsten powder that reduction is processed.
3. the tungsten copper mixed powder is put into stainless steel jar mill, add the Stainless Steel Ball (ratio of grinding media to material 12:1) of 4.8kg, with the lid sealing, be evacuated to 10
-2Pa, pass into again straight argon gas, carry out the high-speed dry mill at ball mill, behind the rotational speed of ball-mill ball milling 15h with 400r/min, in the glove box of argon atmosphere, ball grinder is opened, add 50ml dehydrated alcohol and again sealing taking-up to ball grinder, the rotational speed of ball-mill ball milling 3h with 150r/min obtains the nanocrystalline W-Cu composite powder of high solid solution.
4. the reduction that with ball milling gained powder time of carrying out in atmosphere of hydrogen is 45min is processed, and reduction temperature is 780 ℃.
5. the ball milling ball-milled powder after will reducing is packed into to cooperate closely and at internal surface and is scribbled in the high-strength graphite mould of releasing agent, and wherein releasing agent is boron nitride.
6. mould is put into vacuum hotpressing machine.From rising to 1130 ℃, insulation 20min is cooled to 1070 ℃ with the rate of temperature fall of 3 ℃/min, applies the pressure of 45Mpa with the temperature rise rate of 15 ℃/min, and heat-insulation pressure keeping 1.5h cools to room temperature with the furnace.Whole intensification, insulation, pressurize and temperature-fall period vacuum tightness maintain 10
-3~ 10
-4Pa.
7. the demoulding: the tungsten-copper alloy ingot is taken out from graphite jig, surface finish, according to dense sintering metallic substance and Wimet density inspect method (GB GB03850), recording the actual density of matrix material is 14.18g/cm
3, relative density=actual density/standard density=99.3% can find out that by the back scattering pattern of metallographic its tungsten is evenly distributed mutually, particle diameter is 0.3 ~ 0.7 μ m.
Embodiment 3: the preparation standard composition is W(55%wt), tungsten-copper alloy Cu(45%wt), its standard density is 12.65g/cm
3, follow these steps to finish.
With general industry with pure copper powder (particle diameter is 5 ~ 100 μ m), pure tungsten powder (particle diameter is 2 ~ 15 μ m) respectively take by weighing 260,140g in atmosphere of hydrogen under the time of carrying out be that 30min reduction is processed, reduction temperature is respectively 450 ℃, 780 ℃.
2. will mix 2 hours at mixer through copper powder and the tungsten powder that reduction is processed.
3. the tungsten copper mixed powder is put into stainless steel jar mill, add the Stainless Steel Ball (ratio of grinding media to material 10:1) of 4kg, with the lid sealing, be evacuated to 10
-2Pa, pass into again straight argon gas, carry out the high-speed dry mill at ball mill, behind the rotational speed of ball-mill ball milling 20h with 400r/min, in being full of the glove box of argon atmosphere, ball grinder is opened, add 60ml dehydrated alcohol and again sealing taking-up to ball grinder, the rotational speed of ball-mill ball milling 4h with 180r/min obtains the nanocrystalline W-Cu composite powder of high solid solution.
4. the reduction that with ball milling gained powder time of carrying out in atmosphere of hydrogen is 30min is processed, and reduction temperature is 750 ℃.
5. the ball milling ball-milled powder after will reducing is packed into to cooperate closely and at internal surface and is scribbled in the high-strength graphite mould of releasing agent, and wherein releasing agent is boron nitride.
6. mould is put into vacuum hotpressing machine.10
-310
-4Under the vacuum tightness of Pa, from rising to 1100 ℃, insulation 15min is cooled to 1050 ℃ with the rate of temperature fall of 5 ℃/min, applies the pressure of 40Mpa with the temperature rise rate of 10 ℃/min, and heat-insulation pressure keeping 1.5h cools to room temperature with the furnace.
7. the demoulding: the tungsten-copper alloy ingot is taken out from graphite jig, surface finish, according to dense sintering metallic substance and Wimet density inspect method (GB GB03850), recording the actual density of matrix material is 12.59g/cm
3, relative density=actual density/standard density=99.5% can find out that by the back scattering pattern of metallographic tungsten is evenly distributed mutually, particle diameter is 0.5 ~ 0.8 μ m.
Claims (10)
1. the preparation method of the thin brilliant tungsten-copper alloy of high densification may further comprise the steps:
The first step: starting material prereduction is processed
Get respectively the prereduction in hydrogen atmosphere of pure copper powder, pure tungsten powder, the pure copper powder reduction temperature is: 400 ~ 500 ℃; The pure tungsten powder reduction temperature is: 700 ~ 800 ℃; The mean particle size of pure copper powder, pure tungsten powder is 2 ~ 15 μ m;
Second step: ball milling
The first step gained pure copper powder, pure tungsten powder are mixed, place the ball sealer grinding jar, be evacuated to 10
-1~ 10
-2Then Pa, passes into rare gas element to normal pressure in ball grinder; At first, dry grind at a high speed with the rotational speed of ball-mill of 400 ~ 500r/min after; Add the low molecule grinding aid that accounts for ball, material total mass 0.1 ~ 0.2% again in ball grinder, then, the rotational speed of ball-mill low speed wet-milling with 125 ~ 200r/min obtains the nanocrystalline W-Cu composite powder of high solid solution;
The 3rd step: restore
The nanocrystalline W-Cu composite powder of the high solid solution of second step gained is placed hydrogen atmosphere, be heated to 700 ~ 800 ℃, insulation 0.5 ~ 1.0h restores;
The 4th step: sintering
The 3rd step gained powder is packed in the graphite jig, and it is 10 that mould is put into vacuum tightness
-3~ 10
-4In the vacuum hotpressing machine of Pa, temperature rise rate with 10 ℃/min ~ 20 ℃/min rises to 1100 ~ 1150 ℃ from room temperature, after the insulation, rate of temperature fall with 2 ~ 5 ℃/min is cooled to 1050 ~ 1080 ℃, apply the pressure of 40 ~ 50Mpa, heat-insulation pressure keeping 1.0 ~ 2.0h cools to room temperature with the furnace, namely obtains high fine and close thin brilliant tungsten-copper alloy.
2. the preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification according to claim 1, it is characterized in that: described pure copper powder, pure tungsten powder are technical pure copper powder, technical pure tungsten powder; Its purity is respectively: copper powder purity〉99.7%, tungsten powder purity 99.5%.
3. the preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification according to claim 1 and 2, it is characterized in that: described prereduction soaking time is 0.5 ~ 1h.
4. the preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification according to claim 1 is characterized in that: in the second step, it is to adopt mixer to mix 1 ~ 2 hour that described pure copper powder, pure tungsten powder mix.
5. the preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification according to claim 1 is characterized in that: in the 4th step, described graphite jig internal surface scribbles releasing agent, and described releasing agent is boron nitride.
6. the preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification according to claim 1 is characterized in that: in the second step, the ball material mass ratio of described high speed dry grinding and described low speed wet-milling is: 10 ~ 15:1; Described high-speed dry time consuming 10 ~ 20h; Low speed wet-milling time 2 ~ 5h.
7. the preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification according to claim 6 is characterized in that: in the second step, described low molecule grinding aid is selected from a kind of in dehydrated alcohol, stearic acid, ethylene glycol, the propylene glycol; Low molecule grinding aid is added in the ball grinder, is to place the glove box of atmosphere of inert gases to open ball grinder, add low molecule grinding aid to ball grinder after, ball sealer grinding jar again.
8. the preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification according to claim 7 is characterized in that: in the 4th step, 1100 ~ 1150 ℃ of sintered heat insulating times are 15 ~ 30min; 1050 ~ 1080 ℃ of heat-insulation pressure keeping times are 1.0 ~ 2.0h.
9. the preparation method of the thin brilliant tungsten-copper alloy of a kind of high densification according to claim 8 is characterized in that: the high fine and close thin brilliant tungsten-copper alloy relative density for preparing is 92.5% ~ 99.5%, and tungsten grain is of a size of 0.3 ~ 0.8 μ m.
10. the preparation method of the thin brilliant tungsten-copper alloy of the described a kind of high densification of any one according to claim 1-9 is characterized in that: the high fine and close thin brilliant tungsten-copper alloy of preparation comprises that following component forms by mass percentage:
Tungsten 50 ~ 90,
Copper 10 ~ 50.
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